CN114855203A - Application of perovskite LSCM material in solid oxide electrolytic cell - Google Patents
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- 239000002245 particle Substances 0.000 description 3
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- 229910002161 La0.75Sr0.25Cr0.5Mn0.5O3-δ Inorganic materials 0.000 description 2
- 229910002160 La0.75Sr0.25Cr0.5Mn0.5O3−δ Inorganic materials 0.000 description 2
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910002132 La0.6Sr0.4Co0.2Fe0.8O3-δ Inorganic materials 0.000 description 1
- 229910002131 La0.6Sr0.4Co0.2Fe0.8O3–δ Inorganic materials 0.000 description 1
- 229910002130 La0.6Sr0.4Co0.2Fe0.8O3−δ Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
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- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/042—Electrodes formed of a single material
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
- C25B1/042—Hydrogen or oxygen by electrolysis of water by electrolysis of steam
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/01—Products
- C25B3/03—Acyclic or carbocyclic hydrocarbons
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses an application of a perovskite LSCM material in a solid oxide electrolytic cell. The perovskite LSCM material is La x Sr 1‑x Cr 0.5 Mn 0.5 O 3‑δ Wherein x is more than or equal to 0.5<1, applied to a solid oxide electrolytic cell as a fuel electrode material, has excellent mixed conduction characteristics of oxygen ions and electrons, and can maintain structural stability for a long time in an oxidized or reduced state and in an electrolytic atmosphere of water vapor and carbon dioxide, which is CO 2 And H 2 And in the O co-electrolysis process, the excellent co-electrolysis characteristic and anti-carbon deposition performance are shown.
Description
Technical Field
The invention belongs to the field of solid oxide electrolytic cells, and relates to perovskite La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ Use of (LSCM) material in a solid oxide electrolysis cell.
Background
Solid Oxide Electrolysis Cells (SOEC) are a device for continuously and efficiently converting electrical energy into chemical energy without capacity limitationReceiving wide attention all over the world, the efficiency of electrolytic hydrogen production can approach 100% when operating at high temperature (700-900 ℃), which is far higher than the current mature and gradually commercialized Alkaline water Electrolysis (AEC) and electrolytic water hydrogen production technology (PEMEC). The co-electrolysis technology of the Solid Oxide Electrolytic Cell (SOEC) can not only realize energy storage without capacity limitation, but also convert water and carbon dioxide into fuel. The electrode material of the fuel electrode of a solid oxide electrolysis cell is a bottleneck of the co-electrolysis technology. The water vapor content in the intake air of the fuel electrode (hydrogen electrode) of the SOEC is obviously improved, and the high-temperature and high-humidity environment of the fuel electrode at the moment is easy to cause the agglomeration and coarsening of particles of the traditional metal ceramic fuel electrode, so that the polarization of the fuel electrode is increased [ Pihlatie, M; kaiser, a.; mogensen, m., et al.electric conductivity of Ni-yszcomposities; migration work to Ni particle growth [ J ]].Solid State lonics,2011,189(1):89-90]. Due to CO 2 Due to the existence of the (S), the fuel is easy to generate carbon deposition phenomenon [ Tao, Y; ebbesen, S.D; mogensen, M.B. grading of solid oxide cells reducing co-electrolysis of steam and carbon dioxide at high current mutations [ J].Journal of Power Sources,2016,328:452-462.]. In the process of searching for a proper SOEC co-electrolysis fuel electrode material, perovskite oxide attracts attention due to good catalytic activity and anti-carbon deposition performance, and the general formula of the perovskite oxide is ABO 3 。
The chinese patent CN 105130426B uses a strontium titanate-based fuel electrode material with high temperature chemical stability to replace the Ni-based cermet fuel electrode material, but only improves the structural stability of the material itself at high temperature, and does not improve the carbon deposition prevention capability of the fuel electrode material. Chinese patent CN 102731090A discloses a La and Cr co-doped strontium titanate fuel electrode material which has high ionic conductivity and can be directly used for a hydrocarbon solid oxide fuel cell, but when strontium titanate is used as a matrix as a solid oxide electrolytic cell fuel electrode material, the catalytic capability to carbon dioxide is relatively poor, the polarization resistance is about 50 omega (horse mark. preparation and common electrolytic performance research of a novel ceramic fuel electrode of a solid oxide electrolytic cell [ D ]. Nanjing: Nanjing university of science and technology, 2021:63-64], and the long-term stability of the cell is influenced, so that a fuel electrode material which has good stability in a reducing atmosphere and excellent sulfur and carbon deposition resistance is required to be found.
Disclosure of Invention
The invention aims to provide perovskite La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ Use of (LSCM) material in a solid oxide electrolysis cell.
In particular, the perovskite La of the invention x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is used as a co-electrolysis fuel electrode material of a solid oxide electrolytic cell and is applied to the solid oxide electrolytic cell.
The perovskite La of the invention x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ Material, wherein x is more than or equal to 0.5<1 and delta is the stoichiometric ratio of oxygen vacancies determined by the doping element and the atmosphere in which the material is located.
Preferably, x is 0.75, perovskite-type La 0.75 Sr 0.25 Cr 0.5 Mn 0.5 O 3-δ The material has the best stability and electrical property when used as a co-electrolysis fuel electrode material of a solid oxide electrolytic cell.
The perovskite La of the invention x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is prepared by any one or two of the existing methods, such as a solid phase method, a sol-gel method and a combustion method.
The perovskite La of the invention x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The specific application method of the material as the co-electrolysis fuel electrode material of the solid oxide electrolytic cell comprises the following steps: by a screen printing method, the perovskite La is prepared x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is printed on the electrolyte side of the oxygen electrode/electrolyte semi-electrolytic cell, dried and calcined to form the electrolytic cell.
The oxygen electrode of the invention adopts oxygen electrode materials which are conventionally used in the technical field, such as lanthanum strontium manganate.
Preferably, the thickness of the coating of the fuel electrode is 10 to 70 μm.
Compared with the prior art, the invention has the following advantages:
(1) the invention firstly prepares perovskite type La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is used as a fuel electrode of a solid oxide electrolytic cell, and is an oxide, so that the chemical composition is stable in an oxidation-reduction atmosphere, the structural stability can be maintained in an oxidation or reduction state and an electrolysis atmosphere of water vapor and carbon dioxide for a long time, and the co-electrolysis can be stably and efficiently carried out for a long time;
(2) perovskite type La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material has good catalytic activity on carbon dioxide, and the constructed solid oxide fuel electrolytic cell shows obvious performance advantage and carbon deposition resistance when electrolyzing carbon dioxide or mixed gas of carbon dioxide and water vapor.
Drawings
FIG. 1 is an XRD pattern of LSCM powder prepared by different preparation methods;
FIG. 2 is an SEM image of the interface of an LSCM full cell fuel electrode and electrolyte;
FIG. 3 shows O of LSCM powder at 800 deg.C 2 、H 2 XRD pattern after 10h of medium treatment;
FIG. 4 is a plot of conductivity versus temperature for an LSCM sample under an air atmosphere;
FIG. 5 is a graph of conductivity versus temperature for LSCM samples prepared by different methods of preparation under an air atmosphere;
FIG. 6 is an EIS curve of an LSCM cell loaded with different voltages in an atmosphere of 60% water vapor and 40% carbon dioxide;
fig. 7 is a schematic of the electrolysis process of carbon dioxide and water vapor on LSCM.
Detailed Description
The invention is further described with reference to the following detailed description of embodiments in conjunction with the accompanying drawings.
The LSCM fuel electrode material of the present invention is prepared by using one or two of the existing methods, such as a solid phase method, a sol-gel method, and a combustion method, and reference may be made to the existing documents [ sunkening. solid oxide fuel cell [ M ]. beijing: scientific Press, 2019, page 108-109 ], or Chinese patent application CN 113258086A, or Chinese patent application CN 113178587A, or Chinese patent application CN 113782798A.
Example 1
(1) Perovskite type La 0.75 Sr 0.25 Cr 0.5 Mn0.5O 3-δ The preparation of the material adopts a sol-gel method, and comprises the following specific steps:
according to the ratio of strontium: lanthanum: chromium: manganese 1: 3: 2: 2 molar ratio of La (NO) first 3 ) 3 ·6H 2 O、Sr(NO 3 ) 2 、Cr(NO 3 ) 3 ·H 2 O and Mn (NO) 3 ) 2 ·4H 2 Adding O into aqueous solution of citric acid monohydrate (molar ratio of the citric acid to metal ions is 1: 1.5), stirring by using an oil bath at the temperature of 80 ℃, adjusting the pH value of the solution to be 6 by using ammonia water during stirring, and continuously stirring until the solution is clear. Continuously stirring under the condition of oil bath, wherein the liquid is turbid and slowly changed into a light yellow solution, and finally slowly stirring in a water bath kettle to form sol, and then aging to obtain gel with increasingly poor fluidity. Taking out the beaker, drying at 150 ℃ in a drying oven, finally changing the gel into a solid mixed with organic matters, and then calcining for 6 hours at 1000 ℃ in a muffle furnace to remove the organic matters to obtain LSCM powder.
Fig. 1 is an XRD pattern of the prepared LSCM powder, which shows that the prepared LSCM powder corresponds to a standard peak of perovskite, and XRD patterns of the LSCM powders prepared by the solid phase method and the combustion method are consistent with those of the LSCM powders prepared by the sol-gel method. Fig. 2 is an SEM image of the interface between the fuel electrode and the electrolyte of the LSCM full cell, and it can be seen that the prepared LSCM powder material has small and uniform particles.
A small amount of LSCM powder is taken and treated for 10 hours in oxygen atmosphere and hydrogen atmosphere respectively at the temperature of 800 ℃ simulating the operation of an electrolytic cell. XRD analysis is carried out on the treated LSCM powder, and the result shows that the phase structure of the powder is not obviously changed and no impure phase is generated, so that the LSCM can maintain the structural stability in an oxidation or reduction state for a long time and is a stable electrode material, as shown in figure 3.
(2) Mixing a small amount of prepared LSCM powder sample with 2 wt.% of PVB binder, adding a proper amount of absolute ethyl alcohol for granulation, fully grinding the granulated powder in a mortar, pressing about 2g of powder into strip-shaped test samples with the length, width and height of 20mm, 5mm and 2mm respectively, and placing the samples in a box-type high-temperature sintering furnace for heat treatment at 1400 ℃ for 6 hours. The density of the sample needs to be ensured in the conductivity test, and the density of the sintered sample is above 90%, so that the surface of the strip sample is not cracked or peeled in the pressing process. And then, bonding the conductive silver paste and the silver wires with the sintered body, placing the sintered body into a tubular high-temperature sintering furnace for temperature rise test, selecting a required test atmosphere, controlling the temperature through the tubular furnace, measuring voltage and current at corresponding temperatures by using an electrochemical workstation, and preserving heat for 15min at intervals of 50 ℃, wherein the test temperature range of the sample is 300-800 ℃. FIG. 4 is a graph of the electrical conductivity of LSCM samples as a function of temperature in an air atmosphere, from which it can be seen that the electrical conductivity of LSCM increases with increasing temperature, and at 800 deg.C the electrical conductivity is 16S/cm. Fig. 5 is a graph of the change of the electrical conductivity of the LSCM samples prepared by different preparation methods with the temperature under the air atmosphere, and it can be seen that the difference of the electrical conductivity of the LSCM samples prepared by different preparation methods is small, especially above 700 ℃; for oxide fuel electrodes, sufficient conductivity is present.
(3) LSCM as SOEC fuel electrode material, La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ (LSCF) is an oxygen electrode material, YSZ is used as an electrolyte, the electrode material is brushed on two sides of the electrolyte by a screen printing mode to assemble a single battery, and the thickness of an electrode layer is 30 mu m. H is continuously introduced into the fuel electrode at a flow rate of 30ml/min 2 O and CO 2 The mixture, the fuel electrode, is in a static air atmosphere. The low-frequency and high-frequency sections of the impedance spectrum on the real axis and the intercept of the x axis can obtain the ohmic resistance and the interface polarization resistance of the electrolytic cell under different voltages. Gas transport to electrode-electrolyte-gas three-phase interface at lower voltageThe resistance is very large, most energy of the electric work is not converted into chemical energy at this time, the resistance is represented as the rise of the polarization resistance, at this time, a large amount of Joule heat is generated in the process that current flows through the electrolyte and the electrode to generate voltage drop on the resistance, and the electric work is difficult to be converted into the chemical energy to enable the ohmic resistance to be higher than that under the condition of open circuit. Along with the voltage rise, the polarization resistance is obviously reduced to about 1.5V and 2V, at the moment, the electrolysis process is rapidly carried out, the electric power is rapidly converted into chemical energy, the gas is rapidly reacted and digested in the battery, and the temperature is raised by continuously releasing heat of the electrolytic cell in the voltage rise process, so that the ohmic resistance is promoted to be reduced step by step. At 60% H 2 O+40％CO 2 The current density of the electrolytic cell reaches 0.21A cm under the atmosphere when the voltage is applied for 2V 2 The polarization resistance was about 1.80. omega. cm 2 As shown in fig. 6, the cermet fuel electrode has better initial performance and stability compared to the electrolyte supported SOEC. And for the common electrolysis process, the influence on the high-frequency section polarization resistance is not large under different proportions, and the increase of the total polarization resistance of the electrolytic cell is caused by the increase of the low-frequency section polarization resistance along with the increase of the water vapor concentration, so that the high-concentration water vapor atmosphere can influence the material transmission process of the electrolytic cell. The electrode process for co-electrolysis of carbon dioxide and water vapor on an LSCM fuel electrode is shown in fig. 7. At practical electrolysis voltages, the performance of the electrolysis reaction varies very little at different ratios of carbon dioxide to water vapor. Perovskite type La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material shows excellent anti-carbon deposition performance.
Claims (7)
1. Perovskite type La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ Use of a material in solid oxide electrolysis cells, wherein x is 0.5. ltoreq<1。
2. Use according to claim 1, wherein the perovskite-type La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is used as a co-electrolysis fuel electrode material of a solid oxide electrolytic cell and is applied to solid oxidesIn an electrolytic cell.
3. Use according to claim 1, wherein x is 0.75.
4. Use according to claim 1, wherein the perovskite-type La x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is prepared by any one or two of a solid phase method, a sol-gel method and a combustion method.
5. The application of claim 2, wherein the specific application method is as follows: by a screen printing method, the perovskite La is prepared x Sr 1-x Cr 0.5 Mn 0.5 O 3-δ The material is printed on the electrolyte side of the oxygen electrode/electrolyte semi-electrolytic cell, dried and calcined to form the electrolytic cell.
6. The use of claim 5, wherein the oxygen electrode material is lanthanum strontium manganate.
7. The use according to claim 5, wherein the fuel electrode has a coating thickness of 10 to 70 μm.
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| CN115715985A (en) * | 2022-11-08 | 2023-02-28 | 广东能源集团科学技术研究院有限公司 | Ethanol dry gas reforming catalyst and preparation method and application thereof |
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